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3.2.13 density, g/(cm)3.
3.2.14 thermal conductivity, Wm-1K-1.
3.2.15 t5T(5t ) /T(t ).
12 12
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experiments. The relative standard deviation of the obtained 7.5 Data Recording:
results is a good representation of the random component of the 7.5.1 The data acquisition system must be of an adequate
uncertainty associated with the measurement. Guidelines in speed to ensure that resolution in determining half-rise time on
performing a rigorous evaluation of these factors are given in the thermal curve is no more than 1 % of the half-rise time, for
(6). the fastest thermal curve for which the system is qualified.
7. Apparatus 7.6 Measurement of specimens temperature is performed
The essential components of the apparatus are shown in Fig. using calibrated temperature sensors such as a thermocouple,
4. These are the flash source, specimen holder, environmen- optical pyrometer, platinum resistance temperature detector
tal enclosure (optional), temperature detector and recording (RTD), etc. The temperature sensor shall be in intimate contact
device. with or trained on the sample holder, in close proximity of the
specimen.
7.1 The flash source may be a pulse laser, a flash lamp, or
other device capable to generate a short duration pulse of NOTE 3Touching the specimen with thermocouples is not recom-
mended. Embedding thermocouples into the specimen is not acceptable.
substantial energy. The duration of the pulse should be less
than 2 % of the time required for the rear face temperature rise 7.7 The temperature controller and/or programmer are to
to reach one half of its maximum value (see Fig. 3). bring the specimen to the temperatures of interest.
NOTE 2A pulse length correction may be applied (7, 8, 9) permitting 8. Test Specimen
use of pulse durations greater than 0.5 %.
8.1 The usual specimen is a thin circular disc with a front
7.1.1 The energy of the pulse hitting the specimens surface
surface area less than that of the energy beam. Typically,
must be spatially uniform in intensity.
specimens are 10 to 12.5 mm in diamete (in special cases, as
7.2 An environmental control chamber is required for mea- small as 6 mm diameter and as large as 30 mm diameter have
surements above and below room temperature. been reported as used successfully). The optimum thickness
7.3 The temperature detector can be a thermocouple, infra- depends upon the magnitude of the estimated thermal
red detector, optical pyrometer, or any other sensor that can diffusivity, and should be chosen so that the time to reach half
provide a linear electrical output proportional to a small of the maximum temperature falls within the 10 to 1000 ms
temperature rise. It shall be capable of detecting 0.05 K change range. Thinner specimens are desired at higher temperatures to
above the specimens initial temperature. The detector and its minimize heat loss corrections; however, specimens should
associated amplifier must have a response time not more than always be thick enough to be representative of the test material.
2 % of the half-rise time value. Typically, thicknesses are in the 1 to 6 mm range.
7.4 The signal conditioner includes the electronic circuit to 8.2 Specimens must be prepared with faces flat and parallel
bias out the ambient temperature reading, spike filters, within 0.5 % of their thickness, in order to keep the error in
amplifiers, and analog-to-digital converters. thermal diffusivity due to the measured average thickness, to
less than 1 %. Non-uniformity of either surface (craters,
scratches, markings) should be avoided
8.3 Specimen Surface PreparationIt is a good practice to
apply a very thin, uniform graphite or other high emissivity
coating on both faces of the specimen to be tested, prior to
performing the measurements. The coating may be applied by
spraying, painting, sputtering, etc. This will improve the
capability of the specimen to absorb the energy applied,
especially in case of highly reflective materials. For transparent
materials, a layer of gold, silver, or other opaque materials
must be deposited first, followed by graphite coating. For some
opaque reflective materials, grit blasting of the surface can
provide sufficient pulse absorption and emissivity, especially at
higher temperatures, where coatings may not be stable or may
react with the material.
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when the properties of the reference (including half-rise times 5 0.13879 L 2 /t (2)
and thermal diffusivity values) are similar to those of the
Check the validity of the experiment by calculating at a
unknown and the temperature-rise curves are determined in an
minimum of two other points on the rise curve. The equation is
identical manner for the reference and unknown.
as follows:
9.1.2 An important check of the validity of data (in addition
to the comparison of the rise curve with the theoretical model), 5 k x L 2 /t x (3)
when corrections have been applied, is to vary the specimen where:
thickness. Since the half times vary as L2, decreasing the
tx = the time required for the temperature rise to reach x
specimen thickness by one-half should decrease the half time
percent of Tmax. Values of kx are given in Table 1.
to one-fourth of its original value. Thus, if one obtains the same
thermal diffusivity value (appropriate heat loss corrections 11.1.1 Ideally, the calculated values of for different values
being applied) with representative specimens from the same of x should all be the same. If the values at 25, 50 and 75 %
material of significantly different thicknesses, the results can be Tmax lie within 62 %, the overall accuracy is probably within
assumed valid. 65 % at the half-rise time. If the values lie outside of this
range, the response curve should be analyzed further to see if
10. Procedure thermal radiation heat loss, finite-pulse time or non-uniform
10.1 For commercially produced systems, follow manufac- heating effects are present.
turers instructions. 11.1.2 Thermal radiation heat loss effects are most readily
determined from the temperature of the specimen and the
10.2 The testing procedure must contain the following rear-face temperature response after 4t1/2 by plotting the
functions: experimental values of T/Tmax versus t/t1/2 along with the
10.2.1 Determine and record the specimen thickness. values for the theoretical model. Some numbers for the
10.2.2 Mount the specimen in its holder. theoretical model are given in Table 2.
10.2.3 Establish vacuum or inert gas environment in the 11.1.3 Prepare a display of the normalized experimental
chamber if necessary. data and the theoretical model using the tabulated values of
10.2.4 Determine specimen temperature unless the system T/Tmax and t/t1/2 and the corresponding experimental data at
will do it automatically. several percent levels of the rise. All normalized experimental
10.2.5 Especially at low temperatures, use the lowest level curves must pass through T/Tmax = 0.5 and t/t1/2 = 1.0.
of power for the energy pulse able to generate a measurable Calculations including the 25 to 35 % and 65 to 80 % ranges
temperature rise, in order to ensure that the detector functions are required to compare the experimental data with the
within its linear range. theoretical curve.
10.2.6 After the pulse delivery, monitor the raw or pro- 11.1.4 Examples of the normalized plots for experiments
cessed thermal curve to establish in-range performance. In case that approximate the ideal case, in which both radiation heat
of multiple specimen testing, it is advisable (for time economy) losses and finite pulse time effect exist, are shown in Figs. 5
to sequentially test specimens at the same temperature (includ- and 6, and Fig. 7. Various procedures for correcting for these
ing replicate tests) before proceeding to the next test tempera- effects are also given in Refs. (4, 7-13) and specific examples
ture. are given in 11.2 and 11.3.
10.2.7 The temperature stability (base line) prior and during 11.1.5 The corrections can be minimized by the proper
a test shall be verified either manually or automatically to be selection of specimen thickness. The finite pulse time effect
less than 4 % of the maximum temperature rise. decreases as the thickness is increased, while heat losses
NOTE 4Testing during the temperature program is not recommended decrease as the thickness is reduced.
as it results in lower precision. 11.1.6 Non-uniform heating effects also cause deviations of
10.2.8 Determine the specimen ambient temperature and the reduced experimental curve from the model because of
collect the base line, transient-rise and cooling data, and two-dimensional heat flow. Since there are a variety of non-
analyze the results according to Section 11. uniform heating cases, there are a variety of deviations. Hot
10.2.9 Change or program the specimen temperature as center cases approximate the radiation heat loss example. Cold
desired and repeat the data collection process to obtain center cases result in the rear face temperature continuing to
measurements at each temperature. rise significantly after 4t1/2. Non-uniform heating may arise
10.2.10 If required, repeat the measurements at each tem- from the nature of the energy pulse or by non-uniform
perature on the specimens cooling or on its re-heating over the
same cycle.
TABLE 1 Values of the Constant kx for Various Percent Rises
11. Calculation x(%) kx x(%) kx
11.1 Determine the baseline and maximum rise to give the 10 0.066108 60 0.162236
20 0.084251 66.67 0.181067
temperature difference, Tmax. Determine the time required 25 0.092725 70 0.191874
from the initiation of the pulse for the rear face temperature to 30 0.101213 75 0.210493
reach half Tmax. This is the half-rise time, t1/2. Calculate the 33.33 0.106976 80 0.233200
40 0.118960 90 0.303520
thermal diffusivity, , from the specimen thickness, L, and the 50 ... ... ...
half-rise time t1/2, as follows (1):
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TABLE 2 Values of Normalized Temperature Versus Time for
Theoretical Model
T/Tmax t/t
12 T/Tmax t/t
12
0 0 0.7555 1.5331
0.0117 0.2920 0.7787 1.6061
0.1248 0.5110 0.7997 1.6791
0.1814 0.5840 0.8187 1.7521
0.2409 0.6570 0.8359 1.8251
0.3006 0.7300 0.8515 1.8981
0.3587 0.8030 0.8656 1.9711
0.4140 0.8760 0.8900 2.1171
0.4660 0.9490 0.9099 2.2631
0.5000 1.0000 0.9262 2.4091
0.5587 1.0951 0.9454 2.6281
0.5995 1.1681 0.9669 2.9931
0.6369 1.2411 0.9865 3.6502
0.6709 1.3141 0.9950 4.3802
0.7019 1.3871 0.9982 5.1102
0.7300 1.4601 ... ... FIG. 7 Normalized Rear Face Temperature Rise: Comparison of
Mathematical Model (No Heat Loss) to Experimental Values with
Radiation Heat Losses
1F ~ t ! 5 1G ~ t ! 6 1H ~ t ! 7
where:
values for the coefficients A through H are given in Table 4.
FIG. 6 Normalized Rear Face Temperature Rise: Comparison of Corrected values for thermal diffusivity are calculated from the
Mathematical Model (No Finite Pulse Time Effect) to Experimen- following relation:
tal Values with Finite Pulse Time
corrected 5 0.5 K C /0.13885 (6)
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TABLE 4 Coefficients for Cowan Corrections 12.2.1 Statement that the response time of the detector,
Coefficients Five Half Times Ten Half Times including the associated electronics was adequately checked,
A 0.1037162 0.054825246 and the method used;
B 1.239040 0.16697761
C 3.974433 0.28603437
12.2.2 Energy pulse source;
D 6.888738 0.28356337 12.2.3 Beam uniformity;
E 6.804883 0.13403286
F 3.856663 0.024077586 12.2.4 Type of temperature detector;
G 1.167799 0.0 12.2.5 Manufacturer and model of the instrument used;
H 0.1465332 0.0
12.2.6 Dated version of this test method used.
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14. Keywords
14.1 flash method; infrared detectors; intrinsic thermo-
couples; specific heat capacity; thermal conductivity; thermal
diffusivity; transient temperature measurements
APPENDIXES
X1. THEORY
X1.1 The Ideal CaseThe physical model of the pulse At the rear surface, where x = L, the temperature history can
method is founded on the thermal behavior of an adiabatic be expressed by:
(insulated) slab of material, initially at constant temperature,
whose one side has been subjected to a short pulse of energy.
The model assumes:
T ~ L,t ! 5
Q
CL F `
n51
(
112 ~ 21 ! n exp
2n 2 2
L
t S DG (X1.6)
Two dimensionless parameters, V and can be defined:
one dimensional heat flow; T ~ L,t !
no heat losses from the slabs surfaces; V ~ L,t ! 5 (X1.7)
TM
uniform pulse absorption at the front surface; 2 t
infinitesimally short pulse duration; 5
L2
(X1.8)
absorption of the pulse energy in a very thin layer; TM represents the maximum temperature at the rear surface.
homogeneity and isotropy of the slab material; The combination of Eq X1.6-X1.8 yields:
property invariance with temperature within experimental `
conditions. V 5 112 ( ~ 21 ! exp~ 2n
n 2
! (X1.9)
n51
In deriving the mathematical expression from which the
When V = 0.5, = 1.38, and therefore:
thermal diffusivity is calculated, Parker (1) starts from the
equation of the temperature distribution within a thermally 1.38L 2
5 (X1.10)
insulated solid of uniform thickness L, as given by Carslaw and 2t 1
2
Jaeger (16): or:
1 L L2
T ~ x,t ! 5
L * T ~ x,0 ! dx
0
5 0.1388
t1
(X1.11)
2
1
2 `
(
L n51
exp S
2n 2 2 t
L2 D
cos
n x
L * T ~ x,0 ! cos n Lx dx
0
L where t is the time required for the back surface to reach
12
3 4
sin
T ~ x,0 ! 5
Q
CL
`
112 cos
n51
n x
L ( n g
L
exp S
2n 2 2
L2
t D numbers that vary substantially after using these corrections.
This is understandable, as historically, each investigator has
L
focused on one or another deviation from the ideal model,
(X1.4) while assuming ideality and constancy of the others. This by
where is the density and C is the specific heat capacity of itself is a substantial violation of principles, as in reality all
the material. In this application only a few terms will be parameters vary concurrently, in an extent dictated by the
needed, and since g is a very small number for opaque particular conditions of the experiment. Some situations may
materials, aggravate one condition, for example having a long pulse,
n g n g others may introduce other deviations, such as excessive heat
sin ' (X1.5)
L L losses from the front face due to using very powerful pulses,
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E1461 13
etc. It is therefore incumbent to choose the most proper ably from the one obtained with uniform irradiation. This effect
correction in harmony with the conditions of the experiment can be reduced by increasing the ratio between the specimens
analyzed. thickness and its radius. The same result can be achieved by
The finite pulse width effect, for example, occurs strongly using a temperature measurement system, which automatically
when thin specimens of high thermal diffusivity are tested (2, integrates the signal obtained from the rear face of the
8, 9, 17, 18), while the radiative heat losses become dominant specimen.
at high temperatures (12), when testing thick specimens. In It is a very difficult task to choose the best correction, and
contrast, nonuniform heating can occur during any thermal often not enough information is known about the equipment
diffusivity experiment (19). This can occur when a circular and the testing parameters to do it prudently. In principle, one
surface smaller than the specimen itself is irradiated, or the flux must return to the original premise: the accuracy of the data
density of the pulse varies from point-to-point over the depends on the agreement between the mathematical and
specimens surface. For the same amount of absorbed energy, experimental models. The purpose of applying corrections to
the dimensionless half-max time of the resulting thermal curve the experimental data is to bring it to closer agreement with the
at the center of the rear face of the specimen differs consider- ideal solution by accounting for the aberrations.
X2.1 The fundamental relationship between thermal diffu- X2.1.4 Both reference and unknown specimen must be
sivity (), thermal conductivity (), specific heat capacity (Cp), homogeneous and isotropic, as Eq X2.1 only applies for those
and density (), materials. Heterogeneous and anisotropic materials will fre-
quently produce erroneous data. The process is not purely
5 (X2.1) calorimetric, since the maximum temperature rise is derived
C p
from the signal provided largely by the components with the
allows the calculation of thermal conductivity, a much highest thermal diffusivity, while the internal equilibration may
sought after property, with the knowledge of the other proper- take place after that point in time. For this reason, this method
ties. A method was developed (1) where the specific heat tends to give erroneous results for specific heat capacity for
capacity of a specimen is determined when the thermal materials with large anisotropy (typically composites with an
diffusivity test is performed in a quantitative fashion. Caution ordered directional structure) and for mixtures of components
shall be used in performing this extenstion as errors abounds. with greatly differing thermal diffusivities.
In the course of an ordinary thermal diffusivity test, the amount X2.1.5 The reference and the unknown must be tested very
of energy is important only to the extent that it will generate a close to each other, both temporally (preferably only minutes
sufficient rear face signal. For operating in a calorimetric mode, apart) and thermally (strictly at the same temperature, in the
the energy level must be known closely, controllable and same environment).
repeatable. Approximating adiabatic conditions, the laser pulse
and the detector can be calibrated in unison when a specimen X2.1.6 This being a differential measurement, it is highly
of known specific heat capacity is tested. The measurement desirable to have both reference and unknown tested side-by-
will yield thermal diffusivity, and also a relative measure of side and with very small time intervals in between. It is also
energy expressed in terms of the absolute value of the desirable to test standard/specimen/standard, to minimize er-
maximum attained temperature. By testing an unknown speci- rors from pulse energy variations.
men after this calibration, the specific heat capacity can be
X2.2 The specimens density may be calculated from results
calculated from its maximum attained temperature, relative to
of weight measurements and computed volume. It is appropri-
the one obtained for the standard. There are several conditions
ate to calculate the density at each temperature from the room
that must be satisfied in order for this process to be valid:
temperature density, using thermal expansion data. Consult
X2.1.1 The energy source must be able to reproduce within
Test Method E228 for details.
5 % the energy of a pulse based on the power defining
parameter (charge voltage for lasers, for example) over a X2.3 Thermal conductivity may be calculated using Eq
period of time. X2.1, from the measured values of thermal diffusivity, specific
X2.1.2 The detector must maintain its sensitivity over a heat capacity and density.
period of time without drift, gain change, and within a linear X2.3.1 When measured values of specific heat capacity are
response range. used, the constrains listed under X2.1.1 X2.1.6 also apply to
X2.1.3 The reference specimen and the unknown specimen the resultant thermal conductivity.
must be very similar in size, proportions, emissivity, and X2.3.2 It is permissible to use specific heat capacity and
opacity, to approximate adiabatic behavior to the same extent. density data from other sources than the measurements above.
Both the reference and the unknown specimen should be
coated with a thin uniform graphite layer, to ensure that the X2.4 Reporting specific heat capacity or thermal conductiv-
emissivity of the two materials is the same. ity obtained in this manner must be accompanied by:
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X2.4.1 An accuracy statement determined; X2.4.3 Reference material used.
X2.4.2 The time elapsed between reference and test pulses;
X3.1 Only a few Standard Reference Materials (SRM) are 298 to 1025 K. Its certificate lists an uncertainty of 6 6 %. The
available from the National Metrology Institutes for thermal thermal diffusivity value is determined from the equation:
diffusivity. However, a large amount of data is available in the
~~ mm! 2 s 21 ! 54.406 2 1.35
literature on a number of industry-accepted reference materials
that have been used for verification purposes. 31022 T12.133
31025 T 2 2 1.541 (X3.1)
X3.1.1 A valuable summary and data bank of thermal 31028 T 3 14.147
diffusivity values found in the literature that also provides
310212T 4
recommended values for a wide range of materials, is also
available (20). where T is in K.
5
The sole source of supply of BCR-724 known to the committee at this time is
theInstitute for Reference Materials and Measurements, Retiesweg 11, B-2440 Geel,
Belgium, jrcirmm-rm-sales@ec.europa.eu. If you are aware of alternative suppliers,
please provide this information to ASTM International Headquarters. Your com-
ments will receive careful consideration at a meeting of the responsible technical
committee,1 which you may attend.
REFERENCES
(1) Parker, W. J., Jenkins, R. J., Butler, C. P., and Abbott, G. L., Flash P. H., ed., Plenum Publishing Corp., NY, 1974, p. 287. See also
Method of Determining Thermal Diffusivity Heat Capacity and Sweet, J. N., Data Analysis Methods for Flash Diffusivity
Thermal Conductivity, Journal of Applied Physics, Vol 32, 1961, pp. Experiments, Sandia National Laboratory Report SAND 89-0260,
16791984. (Available from NTIS), February, 1989.
(2) Watt, D. A., Theory of Thermal Diffusivity of Pulse Technique, (12) Clark, L. M., III, and Taylor, R. E., Radiation Loss in the Flash
British Journal of Applied Physics, Vol 17, 1966, pp. 231240. Method for Thermal Diffusivity, Journal of Applied Physics, Vol 46,
(3) Righini, F., and Cezairliyan, A., Pulse Method of Thermal Diffusivity 1975, pp. 714719.
Measurements, A Review, High TemperaturesHigh Pressures, Vol (13) Cowan, R. D., Pulse Method of Measuring Thermal Diffusivity at
5, 1973, pp. 481501. High Temperatures, Journal of Applied Physics, Vol 34, 1963, pp.
(4) Taylor, R. E., Heat Pulse Diffusivity Measurements, High 926927.
TemperaturesHigh Pressures, Vol 11, 1979, pp. 4358. (14) Larson, K. B., and Koyama, K., Measurement of Thermal
(5) Taylor, R. E., Critical Evaluation of Flash Method for Measuring Diffusivity, Heat Capacity and Thermal Conductivity in Two-Layer
Thermal Diffusivity, Revue Internationale des Hautes Temperatures Composite Samples by the Flash Method, in Proceedings 5th
et des Refractaires, Vol 12, 1975, pp. 141145. Thermal Conductivity Conference, University of Denver, Denver,
(6) Taylor, B. N., Kuyatt, C. E., Guidelines for Evaluating and Express- CO, 1965, pp. 1-B-1 to 1-B-24.
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Note 1297, Gaithersburg, MD, 1994. Cooperative Measurements of Heat Transport Phenomena of Solid
(7) Cape, J. A., and Lehman, G. W., Temperature and Finite Pulse-Time Materials at High Temperatures, Advisory Group for Aerospace
Effects in the Flash Method for Measuring Thermal Diffusivity, Research and Development (AGARD), North Atlantic Treaty
Journal of Applied Physics, Vol 34, 1963, pp. 19091913. Organization, AGARD Report No. 606, 1973.
(8) Taylor, R. E., and Clark, III, L. M., Finite Pulse Time Effects in Flash (16) Carslaw H. S., and Jeager, J. C., Conduction of Heat in Solids, 2nd
Diffusivity Method, High TemperaturesHigh Pressures, Vol 6, ed., Oxford University Press, London, 1959.
1974, pp. 6572. (17) Taylor, R. E., and Cape, J. A., Finite Pulse-Time Effects in the Flash
(9) Larson, K. B., and Koyama, K., Correction for Finite Pulse-Time Diffusivity Technique, Applied Physics Letters, Vol 5, 1964, pp.
Effects in Very Thin Samples Using the Flash Method of Measuring 210212.
Thermal Diffusivity, Journal of Applied Physics, Vol 38, 1967, pp. (18) Azumi, T., and Takahashi, Y., Novel Finite Pulse-Width Correction
465474. in Flash Thermal Diffusivity Measurement, Review of Scientific
(10) Heckman, R. C., Error Analysis of the Flash Thermal Diffusivity Instruments, 1981, pp. 14111413.
Technique, Thermal Conductivity 14, Klemens, P. G., and Chu, T. (19) Mackay, J. A., and Schriempf, J. T., Corrections for Nonuniform
K., eds. Plenum Publishing Corp., NY, 1974, pp. 491498. Surface Heating Errors in Flash-Method Thermal Diffusivity
(11) Sweet, J. N., Effect of Experimental Variables on Flash Thermal Measurements, Journal of Applied Physics, Vol 47, 1976, pp.
Diffusivity Data Analysis, Thermal Conductivity 20, Hasselman, D. 16681671.
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E1461 13
(20) Touloukian, Y. S., Powell, R. W., Ho, C. Y., and Nicolaou, M.,
Thermal Diffusivity, Thermophysical Properties of Matter, Vol 10,
IFI/Plenum, NY, 1973.
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